CN101428041A - Cordyceps sinensis extract, preparation method and uses in preparing medicament - Google Patents

Abstract

The invention relates to a cordyceps extract and a preparation method thereof for a preparation, and belongs to the technical field of the extraction and the application of active components from a Chinese traditional medicine. The ultrasonic processing and the extraction method of combining alcohol extraction and water extraction are utilized. The extraction rate of the active components of polysaccharide can be increased by the ultrasonic processing, and since the alcohol extraction and the water extraction are combined, not only the extraction rate of the active components of the polysaccharide can be increased, but also the solvent is saved, the biological activity of the cordyceps polysaccharide is ensured, the utilization ratio of the raw material is increased to the utmost extent, the production cost is reduced, and the invention is suitable for the large-scale industrial production.

Description

A kind of Cordyceps extract, its preparation method and its application in the preparation of medicine

Technical field:

The invention relates to a preparation method of a cordyceps extract and a preparation thereof, which belongs to the technical field of extraction and application of active ingredients of traditional Chinese medicines, and also belongs to the field of traditional Chinese medicine pharmacy.

Background technique:

Cordyceps militaris, also known as Cordyceps militaris, Cordyceps militaris. Cordyceps militaris belongs to Ascomycotina, Clavicipitaceae, Cordyceps. Under the condition that the supply of Cordyceps sinensis is in short supply, Cordyceps militaris, which is as famous as Cordyceps sinensis, has attracted more and more attention in the world. Its development and production have developed new sources of nutrition and medicine for the fields of human health care and medicine. "Compendium of Xinhua Materia Medica" records that Cordyceps militaris is "flat in nature, sweet in taste, beneficial to the lungs and kidneys, nourishing the essence, stopping bleeding and resolving phlegm". Cordyceps militaris has a variety of pharmacological effects: it can lower blood fat, prevent arteriosclerosis, protect heart and brain tissue, calm and hypnotize, enhance macrophage activity, anti-cancer, anti-inflammatory, anti-bacterial, anti-hypoxia, etc.; Cordyceps militaris can be used to treat lung cancer. Emphysema, prostatic hypertrophy; Cordyceps militaris can also improve the body's immunity, assist kidney transplant patients to recover, increase sexual function, etc.

The technical feature of the original capsules and tablets is that the Cordyceps fungus is boiled and alcohol-precipitated to extract various active components of proteins and polysaccharides in the Cordyceps fungus, and the active ingredients are often not completely extracted.

Invention content:

The object of the present invention is to provide an extract of Cordyceps sinensis containing effective active ingredients of Cordyceps sinensis.

The invention also provides its preparation method, which is suitable for industrial production.

The invention also provides the application of the Cordyceps extract in the preparation of medicines, and discloses the corresponding dosage forms of dropping pills, dispersible tablets and slow-release tablets.

Cordyceps extract of the present invention can be obtained by the following methods:

Take the freeze-dried mycelium powder of Cordyceps militaris and 10-30% ethanol and mix them in a ratio of 1:15-40 (W/V), and carry out ultrasonic-assisted extraction at 40-60°C, the ultrasonic frequency is 20-40KHz, and the ultrasonic treatment time is 30- For 90 minutes, repeat the treatment 1-3 times, wherein the ethanol concentration is 10-30%; after the extraction is completed, filter and combine multiple filtrates to obtain filtrate A;

The filter residue is dried, and the ratio of material to water is 1:30-1:50, and it is subjected to ultrasonic treatment (ultrasonic frequency is 20-40KHz) at 40-60°C for 2-4 hours to obtain filtrate B;

Mix filtrate A and filtrate B, concentrate under reduced pressure at 35-45°C and 300-700mmHg, add 95% ethanol or absolute ethanol, make the ethanol weight content in the solution 55-90%, let stand for 8-24 hours, It can be obtained by drying into dry powder with a freeze dryer.

Table 1 Effect of different extraction methods on the extraction rate of Cordyceps polysaccharide

Cordyceps dripping pill method of the present invention comprises the following steps:

Put the Cordyceps extract and base in a ratio of 1 part: (1-9) parts, place in a heating container and heat while stirring until a molten liquid containing the drug extract and base is obtained, and adjust the temperature control of the dropping pill machine system, keep the temperature of the liquid storage bottle of the dropping pill machine at 50°C-90°C, and the temperature of the condensing agent at 5°C-20°C, and wait until the temperatures of the liquid storage bottle of the dropping pill machine and the condensation column are stable to reach the required temperature respectively. At the required temperature state, put the molten liquid containing the Cordyceps extract and the matrix in the liquid storage bottle of the dropping pill machine, and drop it into the condensing agent to form it.

Cordyceps dispersible tablet method of the present invention comprises the following steps:

Crush the Cordyceps extract and auxiliary materials, pass through a 80-200 mesh sieve, take 10-30 parts of Cordyceps extract, add 5-70 parts of disintegrant, 10-85 parts of filler, add 5-30 parts of wetting The binder is made into a suitable soft material, granulated through a 20-40 mesh sieve, dried at a temperature of 40-80°C, sized with a 20-40 mesh sieve, and 1-3 parts are added to the prepared dry granules lubricant, mixed evenly, and tableted to obtain, the preferred tablet hardness is controlled at 4-7kg.

The preparation method of Cordyceps sustained-release tablet of the present invention comprises the following steps:

Take 20.0-60.0 parts of Cordyceps extract, add 10.0-70.0 parts of slow-release material and 5.0-50.0 parts of filler, mix well, pass through 80-120 mesh sieve after crushing; add appropriate amount of adhesive, use dry method Or wet granulation, granulation, adding 1.0 to 3.0 parts of lubricant, mixing evenly, tableting with a tablet machine, to make slow-release tablets containing effective main drug amount.

Compared with the existing extraction method of active ingredients of Cordyceps sinensis, the present invention has the following positive effects: the extraction method combining ultrasonic treatment, alcohol extraction and water extraction is used, ultrasonic treatment can improve the extraction of active ingredients, alcohol extraction and water extraction The combination can not only improve the extraction rate of active ingredients, but also save solvents, thereby ensuring the biological activity of the polysaccharide of Cordyceps, maximizing the utilization rate of raw materials, reducing production costs, and being suitable for large-scale industrial production.

Detailed ways:

Example 1

Take 100g of Cordyceps militaris freeze-dried mycelium powder, add 10~30% ethanol to mix at a ratio of 1:40 (W/V), carry out ultrasonic-assisted extraction at 40°C, the ultrasonic frequency is 40KHz, and the ultrasonic treatment time is 60 minutes, and the treatment is repeated 3 times, wherein the ethanol concentration was 10%, 20%, and 30% respectively; after the extraction was completed, filter, and combine multiple filtrates to obtain filtrate A;

The filter residue was dried, and the ratio of material to water was 1:30, and ultrasonic treatment was carried out at 40°C, the ultrasonic frequency was 30KHz, and the reaction was carried out for 4 hours to obtain the filtrate B;

Filtrate A is mixed with filtrate B, concentrated under reduced pressure at 35-45°C and 700mmHg, adding 95% ethanol or absolute ethanol, making the ethanol weight content in the solution 55%, standing for 24 hours, and making the water-soluble Cordyceps militaris thick The polysaccharide is precipitated; it is obtained by drying into a dry powder with a freeze dryer.

Example 2

Take 100g of Cordyceps militaris freeze-dried mycelium powder and add 10-30% ethanol in the ratio of 1:15 (W/V) to mix, and carry out ultrasonic-assisted extraction at 60°C. The ultrasonic frequency is 20-40KHz, and the ultrasonic treatment time is 90 minutes. Repeat Treat 3 times, wherein the ethanol concentration is respectively 10%, 20%, and 30%; after the extraction is completed, filter and combine multiple filtrates to obtain filtrate A;

The filter residue was dried, and the ratio of material to water was 1:50, and ultrasonic treatment was carried out at 60°C, the ultrasonic frequency was 40KHz, and the reaction was carried out for 3 hours to obtain the filtrate B;

Filtrate A is mixed with filtrate B, concentrated under reduced pressure at 35-45°C and 300mmHg, adding 95% ethanol or absolute ethanol, making the ethanol weight content in the solution 90%, standing for 12 hours, and making the water-soluble Cordyceps militaris thick The polysaccharide is precipitated; it is obtained by drying into a dry powder with a freeze dryer.

Embodiment 3: Cordyceps dripping pills

1. Cordyceps extract: take the Cordyceps extract prepared in Example 1.

2. Preparation method: Take 100 parts of Cordyceps extract, mix it with 100 parts of PEG4000, put it in a heating container and heat it while stirring until the molten liquid containing the drug extract and matrix is obtained, and adjust the temperature control system of the dropping pill machine , heat the liquid storage bottle of the dropping pill machine and keep it at 70°C to 80°C, keep the temperature of the condensing agent at 5°C to 8°C, and wait until the temperature of the condensing agent in the liquid storage bottle and the condensation column of the dropping pill machine reaches the required temperature respectively. At the required temperature state, put the molten liquid containing Cordyceps extract and matrix in the liquid storage bottle of the dropping pill machine, and drop it into the condensing agent simethicone oil to form.

Example 4:

1. Cordyceps extract: take the Cordyceps extract prepared in Example 2.

2. Preparation method: Take 100 parts of Cordyceps extract, mix with 300 parts of Poloxamer 188, place in a heating container and heat while stirring until a molten liquid containing the drug extract and matrix is obtained, then adjust the dropping pill machine The temperature control system makes the liquid storage bottle of the dropping pill machine heated and kept at 70°C-80°C, the temperature of the condensing agent is kept at 5°C-8°C, and the temperature of the condensing agent in the liquid storage bottle of the dropping pill machine and the condensation column When the required temperature states are stably reached respectively, the molten liquid containing the Cordyceps extract and the matrix is placed in the liquid storage bottle of the dropping pill machine, and dropped into the condensing agent simethicone to form.

Embodiment 5: Cordyceps dispersible tablet

Prescription: ingredients (weight percentage content)

20 parts of Cordyceps extract, 32 parts of starch, 15 parts of sodium carboxymethyl cellulose, 10 parts of croscarmellose starch, 15 parts of microcrystalline cellulose, 2 parts of acesulfame potassium, 5 parts of povidone K30 ethanol, micropowder 1 part of silica gel;

Get the Cordyceps extract obtained in Example 1 and the adjuvant in the above prescription and pass through a 100 mesh sieve to pulverize, then mix the Cordyceps extract with sodium carboxymethyl cellulose, cross-linked sodium carboxymethyl starch, microcrystalline cellulose, and starch Mix well, use 5% povidone K30 ethanol solution as a wetting adhesive, make the above solid mixture into a soft material, granulate with a 20-mesh sieve and dry at 60°C, granulate with a 20-mesh sieve, add micropowder silica gel Mix well, control the weight of the tablet, and compress the tablet to obtain the Cordyceps dispersible tablet.

Uniformity inspection of the dispersible tablets obtained in the examples: in water at 20±1°C, the time for them to completely disintegrate and pass through the No. 2 sieve is not more than 140 seconds, which meets the regulations.

The inspection method about the dispersion uniformity and dissolution rate of the dispersible tablet of the present invention is as follows.

1. The inspection of the uniformity of dispersion of the dispersible tablet: check by the requirements of the Chinese Pharmacopoeia 2005 edition two appendix IA dispersible tablet item, get 2 dispersible tablets of the present invention, shake in 100ml water, in 20 ± 1 ℃ of water, 3 Minutes should all disintegrate and pass through the No. 2 sieve, and the device used can be checked according to the requirements of the device under the Chinese Pharmacopoeia 2005 edition, Appendix XA tablet item.

The mensuration of dispersion uniformity of the present invention:

Table 2. Dispersion uniformity inspection results of Cordyceps dispersible tablets

② Dissolution test of dispersible tablets: take this product, and carry out according to the second method of dissolution determination in the second appendix of the Chinese Pharmacopoeia 2005 edition. The rotation speed is 100r/min, the medium is 900ml degassed deionized water, the temperature is 37±0.5°C, 5ml is sampled regularly, filtered through a microporous membrane (0.45um), and deionized water of the same volume and temperature is added at the same time. The subsequent filtrate was tested for polysaccharide concentration by the sulfate anthrone method, and the accumulated release amount was calculated, and the limit was 80% of the marked amount, which should meet the regulations.

Table 3. Comparison of dissolution rates between Cordyceps dispersible tablets and common Cordyceps tablets

From the test data in Tables 1 and 2, it can be seen that the disintegration and dispersion properties of the Cordyceps dispersible tablets fully meet the standards, and the dissolution performance is obviously better than that of ordinary tablets.

Example 6 Cordyceps sustained-release tablet

Prescription: Cordyceps extract 150.0 parts, hydroxypropyl methylcellulose 80.0 parts, ethyl cellulose 67.0 parts,

50.0 parts of microcrystalline cellulose, 3.0 parts of magnesium stearate, 20 parts of 50% ethanol

Preparation method: weigh the Cordyceps extract of the stated amount, add the slow-release material and the filler of the stated amount, mix well, grind them evenly and pass through a 80-120 mesh sieve; add an appropriate amount of binder, adopt wet granulation, and use Sieve with 18 meshes, dry at 40-60°C for 1-2 hours, take out, add the stated amount of lubricant, mix well, and press into tablets with a tablet machine to make slow-release tablets with a tablet weight of 0.5 g.

Example 7

Prescription: Cordyceps extract 150.0 parts, hydroxypropyl methylcellulose 60.0 parts, methyl cellulose 45.0 parts,

92.0 parts of microcrystalline cellulose, 3.0 parts of magnesium stearate, 20 parts of 50% ethanol

Preparation method: weigh the Cordyceps extract of the stated amount, add the slow-release material and the filler of the stated amount, mix well, grind them evenly and pass through a 80-120 mesh sieve; add an appropriate amount of binder, adopt wet granulation, and use Sieve with 18 meshes, dry at 40-60°C for 1-2 hours, take out, add the stated amount of lubricant, mix well, and press into tablets with a tablet machine to make slow-release tablets with a tablet weight of 0.5 g.

Example 8

Prescription: Cordyceps extract 150.0 parts, hydroxypropyl cellulose, 40.0 parts, povidone 25.0 parts,

132.0 parts of lactose, 3.0 parts of magnesium stearate, 20 parts of 50% ethanol

Preparation method: weigh the Cordyceps extract of the stated amount, add the slow-release material and the filler of the stated amount, mix well, grind them evenly and pass through a 80-120 mesh sieve; add an appropriate amount of binder, adopt wet granulation, and use Sieve with 18 meshes, dry at 40-60°C for 1-2 hours, take out, add the stated amount of lubricant, mix well, and press into tablets with a tablet machine to make slow-release tablets with a tablet weight of 0.5 g.

Claims (4)

1, a kind of Cordyceps extract can obtain by the following method:

Get the alcoholic acid mixed proportion of Cordyceps militaris (L.) Link. lyophilizing mycelium powder and 10-30% and count 1:15 ~ 40 by (W/V), 40 ~ 60 ℃ are carried out the ultrasound wave assisted extraction, and ultrasonic frequency is 20 ~ 40KHz, and the supersound process time is 30 ~ 90 minutes, reprocessing 1-3 time, wherein concentration of alcohol is 10 ~ 30%; After extracting end, filter, merge repeatedly filtrate, get filtrate A;

Filter residue and drying is with material-water ratio 1:(30 ~ 50), in 40 ~ 60 ℃ of following supersound process, ultrasonic frequency is 20-40KHz, reacts 2-4 hours, gets liquor B;

Filtrate A is mixed with liquor B, and at 35-45 ℃, concentrating under reduced pressure under the 300-700mmHg adds 95% ethanol or dehydrated alcohol, makes that the ethanol weight content is 55-90% in the solution, leaves standstill 8-24 hour, utilizes freezer dryer to be dried to dry powder promptly.

2, the drop pill made of the described Cordyceps extract of claim 1 is characterized in that:

With claim 1 Cordyceps extract and substrate according to 1 part: the weight proportion of (1～9) part, place that to be heated to fusion in the heating container while stirring standby, the temperature of adjusting drop pill machine reservoir remains on 50 ℃～90 ℃, the temperature of condensing agent remains on 5 ℃～20 ℃, the fused solution that will contain Cordyceps extractum and substrate places in the reservoir of drop pill machine, splashes into molding in the condensing agent.

3, the dispersible tablet made of the described Cordyceps extract of claim 1 is characterized in that:

With claim 1 Cordyceps dry extract and adjuvant drying, pulverizing, cross 80～200 mesh sieves, get 10～30 parts of Cordyceps extracts, add 5～70 parts disintegrating agent, 10～85 parts filler, 5～10 parts of wet adhesives and make soft material, cross the 20-40 mesh sieve and granulate, under 40 ~ 80 ℃ temperature, dry, 20-40 mesh sieve granulate, the lubricant that adds 1～3 part in the dried granule that makes, mix homogeneously, tabletting are promptly.

4, the slow releasing tablet made of the described Cordyceps extract of claim 1 is characterized in that:

Get 20.0～60.0 parts Cordyceps extract drying and crushing, add 10.0～70.0 parts slow-release material and 5.0～50.0 parts filler, mixing is crossed 80～120 mesh sieves after crushed; Add suitable amount of adhesive, adopt dry method or wet granulation, granulate, add 1.0～3.0 parts lubricant mixing, the tablet machine tabletting gets final product.